Abthttb stevens



Re. v16,267

Feb. 16, 1926.

A. STEVENS PROCESS OF SEPARATING BUTYL ALCOHOL AND WATER OriginalFiled March 10. 1920 l gm... Rf

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'im'.riaiarol BUFFALO, NEW. Yong. v

PROCESS OF SEPRATING BUTYL ALCOHOL ,AND WATER. v

riginal No.\1,394,232, datedOctober 18, 1921, Serial No. 364,697, iled March l0, 1920;

reissue led October 9, .1924. Serial- No. 742,672.l

To all whom it may concern.'

Befit 'known that I,V ARTHUR STEVENS, a citizen of the United States, residing at Bulffalo, in the county of Erie and State of New -York,'have invented a new and'u'seful Im provement in Processes of Separating Butyl lcohol and Water, of which the f ollow- ,A ingis a specification.- Thisrinwention relates to a process of se 10 aratingtbutyl alcohol from Water to obtain a 'substantially anhydrous butyl alcohol; 3

"The accompanying'v drawin -shows dia# .grammatically an apparatus y, means of which this process can be carried'out. l@ AIn' the following-description the process will be described as applied to the separation of' water from\ butyl alcohol, but it willbe understood that this process can be used in connection with the separation vof any otherv partly miscible compounds in which the mix-l ture has a boiling point lower than the boil-v ing points of either of the compounds.' Y

'A represents a still or kettle of the kind commonly used in connection with distilling 2i apparatus, and to which thenecessary heat F is supplied by means of a steam coil a, and -B represents the usual lrectifyin column into which the vapor from the still is conducted byI means of a pipe b. The vapor,

30 which passes rthrough kthe rectifier, enters by `means of a` pipe or assa e c into a. artial condenser C, fromw 'cht ecompoun shav- -ingtlie highest boiling points are returned by means of a pipe cfto therecti'fying coll umn B and thevremaining vapors are con-Y ducted by means of a pipe o to a second coii- K denser'D'. All of vthese arts have heretofore been used in connection with distilling apparatus: and the partvof the process in- 40 volving-'the use, of this apparatus is not novel. t

In `the use of this portion of theappa` ratus the still or kettle A is charged with a mixture of butyl alcohol and Iwater vwhich contains approximately 204 per cent of water and 80-per, cent of butyl alcohol, the greaterpart of which has a boiling point of about 90 C. The vapor of constant boiling point mixture which is discharged from the still upon boiling the liquid in the stillmay be said to contain a vapor consisting of approximately 30 per cent water and 70 per cent butyl alcohol boiling at 90 C., and aI quantity of pure butyl alcohol vapor having a higher boiling point. The' Vfunctions 0f the rectifying column B and the partial condenser C are to condense the pure butyl alcohol vapor in excess of the quantity re quired to forni a constant :boiling mixture and to return it to the still A, thus -allowing the vapor of the constant boiling point mixture to pass into the .finalcondenser D, where all theremaining vapor is condensed, forming again a liquid containing butyl alcohol and water, but which contains a larger per- ."centage of Water than the liquid in the still.

' This mixture separates onstanding'as the Application tot butyl alcohol and water are not miscible in the proportions in-which they are present in this mixture. The liquid from the condenser D flows through4 a ipe d through a sight box E where the co' or andyliow of the liquid can be observed. From thel sight box the liquid flows through a pipe e to a f separator F. The liquid reaching the separator will'contain partly a mixture of approximately 20 per cent water and 80 per cent butyl alcohol which is'- the saturation point `-for water in butyl alcohol, and also v a quantity of excesswater. This water contains a' small quantity of butyl alcohol, approximately 4 percent and will collect in the bottom of the separator F, and the mixture v of approximately '2,0 percent water 'and 8O per cent butylalcohol will collect'in the separa-tor F above the other liquid, .which is mostlywater. In orderV to'eect a contin-' uousjseparation of the two liquids in the vseparator,

p a pipe Gr is provided having a `portion g extending-intoproxiinity to the ottom ofthe separator and the other end of which discharges thewater to"a suitable tank or the like P. 'This-mixture of butyl alcohol land water'is drawn' off from the tdp.

of the separator by means Yof a i e H whic can be adjusted to the desired l ,eighty and which conducts the mixture ofV butyl alcohol and vwater to a preheater tank I: Y In this ltank the liquid is preferably heated/.by means of thesteam dischagedv from the steam coils a in the still A, andthismixturein the tank I, which contains-approximately 20 per cent water and 80 returned to the still A throu h a pipe The elimination of Water from t `e separator F through the preheater to the still graduer cent butyl alcohol is ally increases the percentage of butyl alcohol in the still until all the Water has been re-' Eure butyl alcohol passes through the sight ox E, the liquid will be seen to be clear,

the mixture of butyl alcohol 'and water being cloudy, duc to the presence of free particles of water solution of thealcohol in the mixture. Vhen, therefore, vthe temperature atr the head of the rectifying column or the appearance of the stream of liquid in the slght box indicates that the contents of the still are substantially pure butyl alcohol, any one of a number of valves'lc at the top of the rectifying column may be opened, thus permitting pure butyl alcohol to How through the pi e K into the cooler L. By closing a valve in the pipe e, shutting oli the flow of liquid to the separator F, and` opening a valve R in a discharge pipe R2, the pure butyl alcohol may be allowed to flow from the apparatus through the pipe R?. i When the apparatus is charge'dand the tubes in the separator are adjusted to separate the desired compounds the process will be carried on with practically no attention until all of one compound has been separated, after which vthe remaining compound is distilled from the apparatus as described and a new charge is placed in the still. This process greatly reduces the'cost of separa- -tion of compounds of this kind. The continuous process utilizes very eiiiciently the heat in the steam by means of thepreheater in which the mixture is heated before being returned to 'the still. y

I claim as my invention: l

1. The Aprocess of separating `water from a homogeneous aqueous ybutyl alcoholy mixture which comprises distilli-ng the mixture to evolve a constant boiling mixture, condnsing the latter and allowing it to settle in two layers, returning the upper layer to the original mixture undergoing distillation turnin obtained to the still, condensing the constant boiling mixture remaining,'and yallowing it to settle in two layers, Yreturning the upper lalyer to the ori inalliquid undergoing disti lation, ande iminating the lower layer from the process.

, 3. The process, of eliminating the water from a body of homogeneous aqueous butyl alcohol mixture, which comprises distilling water from a the said mixture to evolve a constant boiling` v mixture, condensing the latter and allowing -it to settle into two layers, removing the lower layer, returning the upper layer to the ,main body undergoing distillation, andv thus continuing the distillation until all of the'water is removed andthe body of liquid in the still consists of anh drous butyl alcohol.

4. The 'process o separating water from a mixture containing about 20% water and butyl alcohol, consisting in distilling the mixture to evolve a constant boiling mixture', allowing the same to settle in twov layers,

removing the upper layer comprising a mixture of butyl alcohol and water in the'respective proportions of 80%, and 20% and reit to the still. l

5:.. T ve process of se arating water from amixture containing ab ouslydistilling thefmixture so as to evolve vaporscontaining a constant boiling mix.-y ture of 30% water and 70% butyl alcohol,.

tially'of the constant boiling mixture, sepa;

out 80% butyl alco` .hol and 20% water, consisting in continurately returning to the still the condensate l thus obtained, condensing the constant boiling mixture remaining, and continuously returning to the still the condensate layer having about 80% butyl alcohol therein.

Witness my hand this 22nd day of September, 1924.

ARTHUR STEVENS. 

